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    Process for the preparation and purification of cis-2-methylspiro(1,3-oxathiolane-5,3')quiniclidine hydrochloride
    2.
    发明申请
    Process for the preparation and purification of cis-2-methylspiro(1,3-oxathiolane-5,3')quiniclidine hydrochloride 失效
    顺式-2-甲基螺（1,3-氧硫杂环戊烷-5,3'）奎宁啶盐酸盐的制备和纯化方法

    公开(公告)号：US20090182146A1

    公开(公告)日：2009-07-16

    申请号：US12007394

    申请日：2008-01-10

    申请人： Svetoslav S. Bratovanov ,  Elena Bejan ,  David A. Stradiotto ,  Abbulu Kante ,  Zhi-Xian Wang ,  Stephen E. Horne

    发明人： Svetoslav S. Bratovanov ,  Elena Bejan ,  David A. Stradiotto ,  Abbulu Kante ,  Zhi-Xian Wang ,  Stephen E. Horne

    IPC分类号： C07D497/20

    CPC分类号： C07D497/20

    摘要： An industrially acceptable process for the preparation and purification of cis-2-methylspiro(1,3-oxathiolane-5,3′)quiniclidine from a cisitrans mixture of isomers. Treatment of the mixture with an organic sulfonice acid generates a less soluble acid addition salt that is enriched in the cis-isomer. Recrystallization or pulping using various organic solvents allows for enrichment of the cis-isomer by filtration. These new sulfonic acid salts of the cis-isomer of 2-methylspiro(1,3-oxathiolane-5,3′)quiniclidine prepared according to the present invention could be further converted into the hydrochloride salt by any known procedures such as treatment with a base and then hydrochloric acid salt formation or exchange of the sulfonic acid salt with hydrochloric acid.

    摘要翻译： 从异构体的顺式异构体混合物制备和纯化顺式-2-甲基螺（1,3-氧硫杂环戊烷-5,3'）奎宁啶的工业上可接受的方法。 用有机磺酸处理混合物产生富含顺式异构体的较不溶性的酸加成盐。 使用各种有机溶剂的重结晶或制浆允许通过过滤富集顺式异构体。 根据本发明制备的2-甲基螺旋（1,3-氧硫杂环戊烷-5,3'）奎宁啶的顺式异构体的这些新的磺酸盐可以通过任何已知的方法进一步转化成盐酸盐，例如用 碱，然后与盐酸形成盐酸盐或与盐酸交换磺酸盐。

    Process For The Preparation Of (S)-Alpha-Ethyl-2-Oxo-1-Pyrrolidineacetamide And (R)- Alpha-Ethyl-2-Oxo-Pyrrolidineacetamide
    3.
    发明申请
    Process For The Preparation Of (S)-Alpha-Ethyl-2-Oxo-1-Pyrrolidineacetamide And (R)- Alpha-Ethyl-2-Oxo-Pyrrolidineacetamide 失效
    制备（S）-α-乙基-2-氧代-1-吡咯烷乙酰胺和（R） -

    公开(公告)号：US20090069575A1

    公开(公告)日：2009-03-12

    申请号：US11667824

    申请日：2005-11-21

    申请人： Yuan Qiang Li ,  Zhi-Xian Wang ,  Bhaskar Reddy Guntoori

    发明人： Yuan Qiang Li ,  Zhi-Xian Wang ,  Bhaskar Reddy Guntoori

    IPC分类号： C07D207/12

    CPC分类号： C07D207/27

    摘要： A process provided for the preparation of the (S)— and (R)-alpha-ethyl-2-oxo-1-pyrrolidineacetamide of formula:(1) from (RS)-alpha-ethyl-2-oxo-1-pyrrolidineacetic acid of formula:(2) comprising: i) combining the (RS)-2 with a chiral base (resolving agent) in a resolution solvent and crystallizing from the said mixture the diastereomeric salt of (S)— or (R)-2 and chiral base; ii) regenerating (S)— or (R)-2 from the crystallized diastereomeric salt by treating with a suitable acid or acidic ion-exchange resin; iii) optionally regenerating (R)— or (S)-2 or their mixture (predominantly one enantiomer) from the crystallization mother liquor by treating with a suitable acid or acidic ion-exchange resin; iv) optionally epimerizing (RS)-2 by treating (R)— or (S)-2 or their mixture (predominantly one enantiomer) of step iii with an acid anhydride; V) optionally converting (RS)-2 of step iv into enantiomerically enriched (S)— or (R)-2 through steps i and ii; vi) formation of the mixed anhydride by reacting (R)— or (S)-2 with an alkyl or aryl sulfonyl halogen compound RSO2X in the presence of a suitable base; and vii) reacting the mixed anhydride with ammonia; wherein R represents C 1 to C 15 alkyl or aryl groups such as methyl, ethyl, p-toluenyl, 2,4,6-trimethylbenzyl, 2,4,6-trichloribenzyl, and X represents a halogen atom such as F, Cl and Br atoms.

    摘要翻译： （RS）-α-乙基-2-氧代-1-吡咯烷乙酸的（S） - 和（R）-α-乙基-2-氧代-1-吡咯烷乙酰胺的制备方法 式（2）的酸包括：i）将（RS）-2与分解溶剂中的手性碱（拆分剂）组合并从所述混合物中结晶出（S） - 或（R）-2的非对映体盐 和手性基; ii）通过用合适的酸或酸性离子交换树脂处理从结晶的非对映体盐再生（S） - 或（R）-2） iii）通过用合适的酸或酸性离子交换树脂处理任选地从结晶母液中再生（R） - 或（S）-2或它们的混合物（主要是一种对映异构体） iv）通过用酸酐处理（R） - 或（S）-2或它们的步骤iii的混合物（主要是一个对映异构体）任选差向异构化（RS）-2; V）任选地通过步骤i和ii将步骤iv的（RS）-2转化成对映异构体富集的（S） - 或（R） vi）通过使（R） - 或（S）-2与烷基或芳基磺酰基卤化合物RSO 2 X在合适的碱的存在下反应形成混合酸酐; 和vii）使混合酸酐与氨反应; 其中R表示C 1至C 15烷基或芳基如甲基，乙基，对甲苯基，2,4,6-三甲基苄基，2,4,6-三氯苄基，X表示卤素原子如F，Cl和 Br原子。

    Process for the preparation of (S)-alpha-ethyl-2-oxo-1-pyrrolidineacetamide and (R)-alpha-ethyl-2-oxo-pyrrolidineacetamide
    7.
    发明授权
    Process for the preparation of (S)-alpha-ethyl-2-oxo-1-pyrrolidineacetamide and (R)-alpha-ethyl-2-oxo-pyrrolidineacetamide 失效
    制备（S）-α-乙基-2-氧代-1-吡咯烷乙酰胺和（R）-α-乙基-2-氧代 - 吡咯烷乙酰胺的方法

    公开(公告)号：US07902380B2

    公开(公告)日：2011-03-08

    申请号：US11667824

    申请日：2005-11-21

    申请人： Yuan Qiang Li ,  Zhi-Xian Wang ,  Bhaskar Reddy Guntoori

    发明人： Yuan Qiang Li ,  Zhi-Xian Wang ,  Bhaskar Reddy Guntoori

    IPC分类号： C07D207/12

    CPC分类号： C07D207/27

    摘要： A process provided for the preparation of the (S)- and (R)- alpha- ethyl-2-oxo-1-pyrrolidineacetamide of formula:(1) from (RS)-alpha-ethyl-2-oxo-1-pyrrolidineacetic acid of formula:(2) comprising: i) combining the (RS)-2 with a chiral base (resolving agent) in a resolution solvent and crystallizing from the said mixture the diastereomeric salt of (S)- or (R)-2 and chiral base; ii) regenerating (S)- or (R)-2 from the crystallized diastereomeric salt by treating with a suitable acid or acidic ion-exchange resin; iii) optionally regenerating (R)- or (S)-2 or their mixture (predominantly one enantiomer) from the crystallization mother liquor by treating with a suitable acid or acidic ion-exchange resin; iv) optionally epimerizing (RS)-2 by treating (R)- or (S)-2 or their mixture (predominantly one enantiomer) of step iii with an acid anhydride; V) optionally converting (RS)-2 of step iv into enantiomerically enriched (S)- or (R)-2 through steps i and ii; vi) formation of the mixed anhydride by reacting (R)- or (S)-2 with an alkyl or aryl sulfonyl halogen compound RSO2X in the presence of a suitable base; and vii) reacting the mixed anhydride with ammonia; wherein R represents C 1 to C 15 alkyl or aryl groups such as methyl, ethyl, p-toluenyl, 2,4,6-trimethylbenzyl, 2,4,6-trichloribenzyl, and X represents a halogen atom such as F, Cl and Br atoms.

    摘要翻译： 由（RS）-α-乙基-2-氧代-1-吡咯烷乙酸制备式（1）的（S） - 和（R）-α-乙基-2-氧代-1-吡咯烷乙酰胺的方法 式（2）的酸包括：i）将（RS）-2与分解溶剂中的手性碱（拆分剂）组合并从所述混合物中结晶出（S） - 或（R）-2的非对映体盐 和手性基; ii）通过用合适的酸或酸性离子交换树脂处理从结晶的非对映体盐再生（S） - 或（R）-2） iii）通过用合适的酸或酸性离子交换树脂处理任选地从结晶母液中再生（R） - 或（S）-2或它们的混合物（主要是一种对映异构体） iv）通过用酸酐处理（R） - 或（S）-2或它们的步骤iii的混合物（主要是一个对映异构体）任选差向异构化（RS）-2; V）任选地通过步骤i和ii将步骤iv的（RS）-2转化成对映异构体富集的（S） - 或（R） vi）通过使（R） - 或（S）-2与烷基或芳基磺酰基卤化合物RSO 2 X在合适的碱的存在下反应形成混合酸酐; 和vii）使混合酸酐与氨反应; 其中R表示C 1至C 15烷基或芳基如甲基，乙基，对甲苯基，2,4,6-三甲基苄基，2,4,6-三氯苄基，X表示卤素原子如F，Cl和 Br原子。

    Process for the preparation of phenylcarbamates
    8.
    发明授权
    Process for the preparation of phenylcarbamates 失效
    苯基氨基甲酸酯的制备方法

    公开(公告)号：US07884121B2

    公开(公告)日：2011-02-08

    申请号：US11808430

    申请日：2007-06-11

    申请人： Mohammed Abdul Raheem ,  Zhi-Xian Wang ,  Eckardt C. G. Wolf

    发明人： Mohammed Abdul Raheem ,  Zhi-Xian Wang ,  Eckardt C. G. Wolf

    IPC分类号： A61K31/4172 ,  C07D233/64

    CPC分类号： C07C271/44 ,  C07D233/54

    摘要： This invention relates to a process for the preparation of an aminoalkyl phenyl carbamate compound of formula 1, wherein R1 and R2 independently are hydrogen or C1-6 alkyl; R3 and R4 are the same or different and each is a lower alkyl; or R3 and R4 together with the nitrogen to which they are attached form a cyclic moiety of a three to eight-member ring, with or without a hetero atom like nitrogen or oxygen; R5 and R6 independently are hydrogen, linear, branched or cyclic C1-6 alkyl, allyl, propargyl or benzyl; or R5 and R6 together with the nitrogen to which they are attached form a cyclic moiety of three to eight member ring, with or without a hetero atom like nitrogen or oxygen; the carbon center marked with “*” is racemic or enantiomerically enriched (R)- or (S)-configuration; and pharmaceutically acceptable addition salts, and crystalline and amorphous forms thereof comprising the steps of: i) converting an amine R5R6NH to a carbamoylimidazolium salt of formula 3 wherein R5 and R6 are as defined above; X− is a counterion and R7 is an alkyl or aryl group; ii) reacting in a solvent at a controlled reaction temperature the compound of formula 3 with a compound of formula 4, wherein R1, R2, R3, R4 and “*” are as defined above to give the compound of formula 1; and iii) isolating the compound of formula 1.

    摘要翻译： 本发明涉及一种制备式1氨基烷基苯基氨基甲酸酯化合物的方法，其中R1和R2独立地是氢或C1-6烷基; R3和R4相同或不同，各自为低级烷基; 或R 3和R 4与它们所连接的氮一起形成三至八元环的环状部分，具有或不具有诸如氮或氧的杂原子; R 5和R 6独立地是氢，直链，支链或环状C 1-6烷基，烯丙基，炔丙基或苄基; 或R 5和R 6与它们所连接的氮一起形成具有或不具有诸如氮或氧的杂原子的三至八元环的环状部分; 标记有“*”的碳中心是外消旋或对映体富集（R） - 或（S） - 构型; 和其药学上可接受的加成盐，以及其结晶和无定形形式，其包括以下步骤：i）将胺R5R6NH转化为式3的氨基甲酰基咪唑鎓盐，其中R 5和R 6如上所定义; X-是抗衡离子，R7是烷基或芳基; ii）在受控反应温度下在溶剂中使式3化合物与式4化合物反应，其中R 1，R 2，R 3，R 4和“*”如上所定义，得到式1化合物; 和iii）分离式1的化合物。

    Process for the preparation of phenylcarbamates
    10.
    发明申请
    Process for the preparation of phenylcarbamates 失效
    苯基氨基甲酸酯的制备方法

    公开(公告)号：US20070207990A1

    公开(公告)日：2007-09-06

    申请号：US11365596

    申请日：2006-03-02

    申请人： Zhi-Xian Wang ,  Stephen Horne ,  K.S. Murthy

    发明人： Zhi-Xian Wang ,  Stephen Horne ,  K.S. Murthy

    IPC分类号： A61K31/553 ,  A61K31/551 ,  A61K31/5375 ,  A61K31/495 ,  A61K31/445 ,  A61K31/421 ,  A61K31/4174 ,  A61K31/40 ,  A61K31/397 ,  A61K31/396 ,  A61K31/325

    CPC分类号： C07C269/04 ,  C07C271/44

    摘要： A process for the preparation of aminoalkyl phenyl carbamate compounds of Formula I, wherein R1 and R2 independently are hydrogen or a C1-6 alkyl; R3 and R4 are the same or different and each is a C1-6 alkyl; or R3 and R4 together with the nitrogen to which they are attached form a cyclic three to eight membered ring, with or without a heteroatom like nitrogen or oxygen; R5 and R6 independently are hydrogen, linear, branched or cyclic C1-6 alkyl; or R5 and R6 together with the nitrogen to which they are attached form a cyclic three to eight membered ring, with or without a heteroatom like nitrogen or oxygen; the carbon centre designated “*” can be racemic or enantiomerically enriched in the (R)— or (S)-configuration; and pharmaceutically acceptable acid addition salts thereof.

    摘要翻译： 制备式I的氨基烷基苯基氨基甲酸酯化合物的方法，其中R 1和R 2独立地是氢或C 1-6烷基， 烷基; R 3和R 4相同或不同，各自为C 1-6烷基; 或R 3和R 4与它们所连接的氮一起形成具有或不具有杂原子如氮或氧的环状三元至八元环; R 5和R 6独立地是氢，直链，支链或环状C 1-6烷基; 或R 5和R 6与它们所连接的氮一起形成具有或不具有杂原子如氮或氧的环状三元至八元环; 指定为“*”的碳中心可以是（R） - 或（S） - 构型的外消旋或对映异构体富集; 及其药学上可接受的酸加成盐。